Potassium Hydroxide → (-)-3-t-Butyldimethylsilyloxybutyric acid

HRID 1090327노트

반응식

HRID 1090327 반응식
[Si:1]([O:8][CH:9]([CH3:15])[CH2:10][C:11]([O:13]C)=[O:12])([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2].[OH-].[K+]>CO>[Si:1]([O:8][CH:9]([CH3:15])[CH2:10][C:11]([OH:13])=[O:12])([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2]

참가 물질

4

반응물 2

HCID 14797Potassium HydroxideHCID 137127793-(tert-Butyldimethylsiloxy)butyric acid methyl ester

생성물 1

HCID 13712781(-)-3-t-Butyldimethylsilyloxybutyric acid수율 95%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of 3.58 g (15.4 mmol) of methyl (-)-3-t-butyldimethylsilyloxybutyrate dissolved in 30 ml of methanol, 30 ml of 1N potassium hydroxide was added and the mixture was stirred for 15 hours. After almost all methanol was distilled away, the resultant was acidified with 1N hydrochloric acid and extracted with diethyl ether. The extract was washed with a saturated solution of NaCl, dried with anhydrous magnesium sulfate and concentrated under reduced pressure to give 3.18 g of (-)-3-t-butyldimethylsilyloxybutyric acid (yield: 95%).

후처리

  1. distillationAfter almost all methanol was distilled away
  2. extractionextracted with diethyl ether
  3. washThe extract was washed with a saturated solution of NaCl
  4. dry with materialdried with anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-bcb5c6e0d3654d4cb57ce5f4e68ec316
출처 데이터셋
uspto-grants-1992_01
특허 번호
US05081238

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